Preparation of caoutchouc.



' 15=- obtained from essential oils, or by synthet- I 40 ties which are likewise soluble interpineol or removing the precipitates in succession.

I 55 precipitating .agents, which aremerely cheapnnrrnn srArns PATENT OFFICE; .aueus'rnr1xIER, -or.m1ns, FRANCE, ASSIGNOR (114) Les rnonurrs GHMIQUE be cnolssY (I. 'YBASLER & 00. F ramsrrarrce.

. ,PREPARATION or;:eaoo:rcnouc.

m 924,117; Specification or T0 all'whom it ma concern; )1

Be it t "at I,- Aueusrn'lrxmn, chemist; of 82 Rue St. Lazare,- Paris,'in the Repnblic of France, have invented certain- 5 .new and useful'lmprovements in the-Pre aration of Oao'utchouc,. of-which the-following .is a specification. a f Thls inventiom relates to the preparation :of caoutchouc from'rubber Waste -,crude rub-w '10 her or other materials containing =caout-- chouc, and to the purification and' improve-t.

'ment of the quality of caoutchouc. I have discovered that-terpineol; :(either of the liquid orsolid variety, and-whether .ical manufactnrehiand. other oxygen derive tives of the terpinic hydrocarbonsanalogous to terpineo said derivatives having a melt-- ing' point below l50 degrees C. possess aremarkable solvent-- ower on -cadutchouc,-.:

which they dissolve -s owly in the 'cold', but more rapidly 'withthe aid of' heat *and I s have further discovered that =eaoutchouomay be recovered from its terpineoi solution 25. in a high state ofpurity, possessing thereq ui site, qualities of supplenessand-elasticlty, 'and carilableofbeing vulcanized. By t e employment of terpineol or such 7 other analogous-oxygen derivative .of the su terpinic hydrocarbons as a solvent for the purpose stated,-'Which is the essential feature of my invention, 1 am able-to prepare con-- centrated solutions of. cao'utchouc at mod- 'erately low. temperatures, thecharacteristic; hysical qualities of the cadutchouc obtained emg unaffected, .while-im urities -such as mineral matters, tissues an the like insol uble in iierpiineol or the like o'an'be removed .by filtration or decantation: Y Other impuriw the like can be removed by-addingcliqnidsmiscible 'with terpineol and.- which preci i i tate impuritieswithout precipitating t 1e caoutohouc, .or conversely by adding liq- .uids miscible with terpineol-whiehprecip1-- -t'ate the caoutchouc and-leave im 'urities insolution. Or lmay combinebot methods for therelnov'al of soluble impurities-by add ing .both' orders of precipitating-agents and .I" Of the first order'of-preci itating agentsi benzene is the .type,and' of t e second order alcohol or'acetone; but Ido not limit my invention to the employment of. these specific Letters Patent. -Patented J'une'8, -'1 909,

7 h man men :NovemberfiO leoefl semi mi. 45,618.

and convenient types. The selection: of the precipitatingtagent-iand theiexact' order of -prooedurei-to be! followed .depend,'.as-jwill be readily understood, on the nature andiquantit ofimpuritiespresent.

x y dissolving the-waste on impure rubber or other mater al containingcaoutchonc in terpineol :or the'like as described .and separities as-enplainedfli ant enabled to obtain a -caoutchoue of great technical value free from substances which have 1 existed in the best r-ubbers ihitherto obtainable. These substances can be :Iseparated' by tl1e -e1nployment ofthe-newimenstruum iasdescribed. a As an-example of theuregeneration of caoutchoucfront vulcanized rubber waste I proceed as"fol-lows::'-Therubber scraps are hred-uced to .apulp by i suitable mechanical ,mean-s and thendlgestednt a temperature of 100 to 150 0., in a.clpsed digester. provided 'with a stirring arra 'ementgiwith a. sullicient two parts of. terpineo to .onepartof scrap. When the solution ot the caoutchouc 13 complete, 4 or 5 volumes otbenzenearezadded preferably .whilethe. caoutchouc solution is in the digesteriand,thoroughly stirred, and the mixture is them either. filteredsor left to recipitate and the clear liquid decanted ofl'. rom the clear-liquors thenbenzene is rc- --m ovedby v distillationmnd to thegumlny torpineolsolutionalcohol :or acetone. is i add ed, with constant stirring, until the whole of the caoutchouc is-precipitated as aagununy homogeneous masszu The liquid poured oii an dthe mass washed with the uncut- -chouc precipitating agent until it is tree from i te-rpin'eol and it isifinally washed with warm water-and-dried'u. The caoutchouc thus obtained can be vulcanized and loaded or not in the usual way, accordiiu to requirement.

other precipitatim agent employedcan be recovered'by distillation and returned to the manufacture. he terpineolor; .other-omygen derivative ofthe terpinio ihydroearbons employed as a caoutchou'c solvent ms before descr bed has the ellect -ofdevuloanizing theeaoutchouc --when waste rubber or-vulcanized .cad utchouc spondingly valuable in .thisrespect. "---The purification of onoutchquc by the mvention' will be understood tram. the. flo'regoistreaterh and theprocessris therefoneicorrefl rating the. caoutchouc. tronr dissolved iinpu- I quuntityi of-terpineo ay for example about i The terpineol or the lilie'. and the alcohol or 7 ing descri tion, the caoutchouc to be purified being sub ected to'substantially similar treatment.

In carrying out my invention for the recovery or preparationof caoutchouc I may also incorporate for the purpose of improving the quality of the caoutchouc or giving it a special character, gums, such as copal, or like rivative having a melting substances which are soluble in terpineol or oxygen terpinic derivatives analogous thereto. For this purpose a solution of these substances in terpineol or the like may be added to the terpineol or like solution of caoutchouc before precipitation of the latter.

What I claim and desire to secure by Letters Patent is 1. A process of preparing eaoutcho uc, comprising extraction of material containing the same with an oxygen derivative of a terpinic hydrocarbon said derivative having a melting point below 150 degrees C.

2. A process of preparing caoutchouc from rubber waste, comprisin extraction of said waste with an oxygen erivative of a terpinic hydrocarbon said derivative having a melting point below 150 degrees C.

3. A rocess of pre aring caoutchouc from materia containing t e same, comprising the extraction of said material with an oxygen derivative of a terpinic hydrocarbon said deoint below 150 degrees C. and separation o the caoutchouc from other dissolved matter in the solution by a liqui recipitating agent miscible with said derivative.

4. A rocess of preparing caoutchouc from materia containing the same, comprising extraction of said material with an oxygen derivative of a terpinic hydrocarbon said derivative having a melting oint below 150 degrees C. and separation o the caoutchouc from other dissolved matter in the solution by a liquid eaoutchoue precipitating agent miscible with said derivative.

5. A process of preparing caoutcliouc from rubber waste, comprisin extraction of said waste with an oxygen erivative of a terpinic hydrocarbon, said derivative having a melting point below 150 degrees C. and se aration of the caoutchouc from other is? solved matter in the solution by a liquid precipitating agent miscible with said derivative.

6. A process of preparing caoutehouc from rubber waste, C-OIIIPIISlH extraction of said waste with an oxygen derivative of a terpinic hydrocarbon, said derivative having a melting point below 150 degrees C. and separation of the caoutchouc from other dissolved matter in the solution by a liquid 7 caoutehouc precipitating agent miscible with said derivative.

7. A process of preparing caoutehouc C0111- prising the extraction of material containing the same with terpineol.

8. A method or process of preparing caoutchouc from rubber waste, comprising the extraction of said waste with terpineol.

9. A )rocess of pre aring caoutchouc from materia containing the same, comprising the extraction of the material with terpineol, and separation of the caoutchouc from other dissolved matter in the terpineol solution by a liquid precipitating agent miscible with terpineol.

10. A process of preparing caoutchouc i'rom rubber waste, comprising the extraction of the waste with terpineol, and separation of the caoutchouc from other dissolved matter in the terpineol solution by a liquid precipitating agent miscible with terpineol.

11. A process -of preparing eaoutchouc from material containing the same, eomprising extraction of the material with terpineol and precipitation of the caoutehoue from the terpineol solution by a liquid precipitating agent miscible with terpineol.

12. A process of reparing caoutchouc from material containing the same comprising the extraction of the' material with terineol and precipitation of the eaoutchoue rom the terpineol solution by alcohol.

13. A process of preparing caoutchouc from rubber waste, comprising extraction of the waste with terpineol and precipitation of the caoutchouc from the terpineol solution by alcohol.

14. A process of obtaining caoutchouc from material containing the same, comprising extraction of the material with terpineol and precipitation of dissolved matter other than caoutchouc from the terpineol solution by a liquid precipitating agent miscible with terpineol.

15. A process of preparing caoutchouc from rubber waste, comprising extraction of the waste with terpineol and preci )itation of dissolved matter other than caoutc 10110 from the terpineol solution by benzene.

16. process of obtaining caoutchouc from material containing the same, comprising extraction of the material with terpineol and precipitation of dissolved matter other than eaoutehouc from the terpineol solution by benzene.

17. A process of preparing caoutchouc from material containing the same, comprising extraction of the material with terpineol, precipitation of dissolved matter other than caoutchouc in the terpineol solution by a liquid precipitating agent miscible with terpineol, and subsequent precipitation of the caoutchouo by a 11 uid caoutchouc precipitating agent miscible with terpineol.

18. A process oi preparing caoutchouc [rom rubber waste, comprising extraction of the waste with terpineol, precipitation of dis solved matter other than caoutchouc by benzene, distilling oil' the benzene and precipitating the caoutchouc with alcohol.

lOO

ll(l

1 9. In a method or process of preparing caoutchouc from material-- containing the same by means of extraction with an oxygen derivative of a terpinic hydrocarbon, said derivative having a'meltini point below 150 degrees C. the addition to t e caoutchouc solution of other gummy material soluble in said derivative.

20. In a method or process of preparing caoutchouc frommaterial containing the same by means of extraction with terpineol the addition to the terpineol solution of other gummy material soluble in terpineol.

21. In a method or process of preparing caoutchoucfrom rubber waste by means of extraction with terpineol, the addition to the I terpineol solution of caoutchouc' of a terpine'ol solution of copal.

22. Asa new composition of matter, a solution of caoutchonc in an oxygen derivative of a terpinic hydrocarbon said derivative canized caoutchouc free from substances insoluble in a-mixture of terpineol with benzene, other than the vulcanizing or a loading agent.

In witness whereofll have hereunto si ned my name in the presence of two subscri ing witnesses.

AUGUSTE TIXIER.

Witnesses? JOSEPH SmsoN; JOSEPH BASLER. 

